Catalyst for the production of ammonia and process of making the same.



,1. an? are 11 mum w. DE AH'N, or New YonK, N. Y., ASSIGNOR T0 GENERAL CHEMICAL COMPANY, or NEW YORK, N. Y., A CORPORATION or NEW YORK.

CATALYST non THE PRODUCTION or Ammonia AND PROCESS or MAKING THE SAME.

Specification bf Letters Patent.

Patented June 15, 1915.

No Drawing. Original application filed August 2, 1918, Serial No. 782,696. Divided and this application filed June 80, 1914.

To all whom it may concern Be it known that I, FREDRIK W. on JAH a subject of the King of Norway, and a resident of the borough of Manhattan, city, county, and State of New York, have in vented certain new and useful Improvements in Catalysts for the Production of Ammonia and Processes of Making the Same, of which the following is a specification.

My invention relates to the synthetic production of ammonia and more particularly to a new catalytic agent therefor, its production and use. t

The present application is a division of my pending application Serial No. 782,696, filed August 2, 1913. I have discovered that if a gaseous mixture containing nitrogen and hydrogen is suitably passed over a material containing nickel, iron, or molybdenum and'sodium or potassium, and nitrogen, the nitrogen and hydrogen of the gaseous mixture are united to form, ammonia.

When nickel, sodium and nitrogen are used as the catalytic agent, such agent is preferably prepared by suitably placing nickel nitrate on pumice stone, then heating the result to about 550 0., then treating it with hydrogen at about the same temperature and then treating with metallic sodium and subsequehtly with dry ammonia gas at a temperature of about 450 C. With a catalytic agent so prepared nitrogen and hydrogen may be caused to combine with the production of ammonia at a temperature of about 500 C. and a pressure of about 70 atmospheres. i

In order that my invention may be clearly understood, it is now set forth in the form of a specific example, it being understood of course that the invention is not to be limited to the exact materials or proportions thereof nor to the other conditions of the example, since these may be varied without departing from my invention.

EwampZe IPrepa1-z'ng the catalgjzen- Pumice stone in small pieces is purifiedby treatment with hydroch oric acid'in the cold for about twenty-four hours, it is then washed with distilled water until free from chlorid and then ignited to dryness. Of this product 175 grams are treated with 257 grams of crystallized nickel nitrate dissolved in the necessary quantity of water and the Serial No. 848,167.

whole is evaporated to dryness, being stirred thoroughly during the evaporation; in this way the nickel nitrate is to be uniformly distributed over the pumicel The thus treated pumice is now ignited to about 550 C. until fumes are no longer given off and is then heated to about 550 C. in an atmosphere of hydrogen for eight hours or thereabout, i. 6., until water is no longer formed. To the product when cooled 20 grams of metallic sodium are added in an indifferent atmosphere such as thatof hydrogen, the material is heated for the purpose of melting the sodium and the molten metal is uniformly distributed, as by vigorous stirring, over the surfaces of the pumice material. The indifferent gas is then displaced by anhydrous ammonia vapor or gas and the material is heated to about 450 C. until a practically constant weight is obtained thereby introducing nitrogen into the catalyzer. The material after being cooled is sodium and the subsequent treatment with ammonia, sodium amid may be used. I have further found that in the above Example I I can use ferric nitrate, or molybdenum chlorid, in place of the nickel nitrate and potassium in place of the sodium and thus obtain effective catalytic material for the production of ammonia as given'in Example II herein. It is, of course, understood that the catalyzer may cont-aineither nickel, iron, or molybdenum, together with sodium or potassium and nitrogen, or may contain two or more of these metals together with sodium or potassium and nitrogen.

E wample lI-Utz'li2ing the catalyzer to produce anwnom'w.For=producing ammonia about 134 grams of the above catalyzer, ora preferably containing one volume of nitrogen for every three volumes of hydrogen. The gas mixture must be suitably purified and must be freed especially from contact poisons in the well known manner. With the pressure of the gas traversing the chamber within the range of 80 to 90 atmospheres and the temperature of treatment approximately between 520 C. and 540 (3., I have succeeded in producing synthetic ammonia to the extent that the ammonia gas leaving the treating chamber constituted 4.5% by volume of the total gas leaving said chamber. The ammonia is removed from the gas discharged from the catalytic chamber in any suitable manner. I have found that iron, and molybdenum are the equivalents of nickel for the purposes of this invention.

I claim:

1. As a new article of manufacture a substance containing nickel, sodium and nitrogen and which can cause nitrogen and hydrogen to combine to produce ammonia.

2. As a new article of manufacture asubstance obtainable from metallic nickel, metallic sodium and ammonia and containing nickel, sodium and nitrogen and which can cause nitrogen and hydrogen to combine to produce ammonia.

3. The herein described rocess of making a catalytic agent suitable or producing ammonia, whibh comprises treating nickel oxid with hydrogen, adding thereto metallic sodium and treating the .product thus formed with ammonia.

' with ammonia.

4. The herein described rocess of making a catalytic agent suitable or producing ammonia from a mixture of nitrogen and hydrogen, which comprises. treating nickel oxid with hydrogen, adding thereto metallic sodium and treating the product thus formed 5. The process of making a catalytic agent suitable for producing ammonia, which comagent suitable for producing ammonia from nitrogen and hydrogen, which comprises forming a mixture of nickel and sodium and treating the mixture with ammonia.

7.. The process of making a catalytic agent suitable for producing ammonia, which comprises adding to nickel the product resulting from treating sodium with ammonia at an elevated temperature.

8. The process of making a catalytic agent suitable for producing ammonia from nitrogen and hydrogen which comprises adding to nickel the product resulting from treating metallic sodium with ammonia at an elevated temperature.

In testimony whereof I have'hereunto set my hand in the presence of two subscribing witnesses.

FREDRIK W. DE J AHN. Witnesses:

J oHN-A. FERGUSON, FRED A. KLEIN. 

